Panalytical XPert Powder X-Ray Diffraction SOP

Panalytical XPert Powder X-Ray Diffraction SOPTable of ainingSample PreparationPre-OperationSample LoadingRunning a MeasurementTo Stop a Scan in ProgressSample UnloadingPost-OperationConverting DataSafety1.1High Voltage This machine uses high voltages, especially to generatethe X-ray beam. Do not touch any parts of the machine aside from thosespecifically mentioned in this SOP.1.2X-rays X-rays are a very harmful form of radiation and care should betaken to minimize exposure. The radiation material MUST be reviewedprior to training or use of this machine. Additionally, all users MUST haveobtained their X-ray badge prior to use or training on this machine. YourX-ray badge MUST be worn at all times during operation and only thosewearing X-ray badges should be permitted in the room.1.3Moving Components This machine has heavy moving parts. Althoughthese parts only move inside the machine while the X-ray is on (and thusould be taken to ensure you donot get in the way of a moving part.

2.03.0Training2.1Training for this machine is scheduled on demand. Please use the RSCwebsite to request training if you would like to use the machine.2.2Prior to training, users MUST review safety information about X-rays andobtain an X-ray dosimetry badge. The training slides are available whenyou sign up for training and the dosimetry (X-ray) badge application isavailable in the Docs section of the RSC website.Sample Preparation3.1This tool can only measure polycrystalline materialsCAUTIOCAUTION sweeps across a singleThe detector canNburn out if a measurementcrystal peak. If your measurement burns out the detector, yourPI/advisor will be charged for the repair3.2Samples should be loaded on a glass (not quartz) slide3.2.1 The glass slide will not introduce too much additional signal3.3If measuring a powder, use double-sided tape to create a thin layer ofpowder in the middle of your glass slide3.4If measuring a sample, the sample can sit directly on the glass slide (noneed for tape as it will not move)3.5We have aluminum holders you may also use, these are to remain in thelab, and should be cleaned after each use. Please ask for assistance if youneed to use the aluminum holders.3.6The sample needs to be height-matched when loaded so that the top ofthe sample is at the focal point of the X-ray beam3.6.1 For powder samples, a section of single-sided tape on the loadingend is sufficient3.6.2 For larger samples, an additional dummy sample of similar heightwill need to be loaded into the clip.CAUTIONCAUTIONSome signal may come from this dummy sample, soensure that it is not single crystal as well.

4.0Pre-Operation4.1Ensure you have a reservation or that no one will have a reservationduring your time.4.2Ensure that the angles displayed on the front of the machine are theproperAngle displays on the front of the machine.4.3Ensure that the system is at standby power by checking the voltage andcurrent on the front of the toolStandby PowerFull PowerVoltage45kV45kVCurrent20mA40mA4.3.1 X-ray source voltage should be 45kV4.3.1.1If the voltage is not 45kV, do not use the tool. Pleasesend an email to rscinfo@mail.ufl.edu4.3.2 X-ray source current should be 20mA (standby current)4.3.2.1If the current is higher than 40mA or lower than20mA, do not use the tool. Please send an email torscinfo@mail.ufl.edu4.3.2.2If the current is between 20mA and 40mA, themachine can still be used, but please send an email torscinfo@mail.ufl.edu with the time, date, and details4.3.3 If you are using the machine IMMEDIATELY after another user,they may leave the system at full power for you. Otherwise, themachine must be brought to standby power after measurementsare finished.

Indicator on the front of the machine showing the source voltage and current at standbypower.4.4Log in to the TUMI system at the laptop computer4.5The Data Collector software should be left running. If it is not, followthese steps to get it running4.5.1Data Collector and Viewer programs in the Windows bar.4.5.2 Login with the username and password posted on the PC4.5.2.1Username: class4.5.2.2Password: class14.5.3 Select Instrument - Connect4.5.44.5.5 Same config4.5.64.6Once the software is running, raise the system power to full (40mA)4.6.1 Double click the current in the left window4.6.2 Increase the Current by 5mA and select “Apply”4.6.3 Double check on the front of the machine thatthe current was raised4.6.4 Let the Machine saturate at this level for 30-45 seconds.4.6.5 Repeat until you reach 40mA (full power) Select “OK” to closeInstrument settings window.

4.6.6 Double check on the front of the machine that the current wasraised to 40mARaise the current to 40mA in 5mA intervalsThe machine should now read full power.5.0Sample Loading5.1Before opening the door, ensure that the X-ray is blocked5.1.1 The doors should be locked if the X-ray is not blocked, but use theindicator on the front of the tool to be sureThe shutter is closedThe shutter is openThe X-ray is blockedThe X-ray is NOT blockedSafe to openNOT safe to open

5.1.2 Open the doors by sliding each outward5.1.2.1The doors are heavy, so do this slowly and carefully5.1.3 Insert your sample into the spring-loaded clipPicture of a loaded sampleDiagram of loading a larger sample5.1.4 Close the doors slowly and ensure they are completely closed

6.0Running a Measurement6.1To edit your scan parameters, select File - Open Program6.2Select the program you wish to use: Powder Th-2Th Basic Scan- This is the basic scan type(previously “use this program”) It works best for infinitely thicksamples, or phase ID scans of any thickness. Powder Th-2Th fixed -10mm- This scan is a basic powder scanutilizing the programmable slits to maintain a 10mm irradiatedlength on your sample. This can correct for the constant volumeassumption and allow refinements to be used. (Quantitative) Powder Th-2Th fixed- 5mm- Same as 10mm program, justshorter irradiated length on sample. Thin Film 2Th-omega scan- This program runs a 2Theta-omegascan (powder scan) with an omega offset, and a constantirradiated length of 6mm on your sample. This can help scanpolycrystalline thin films on a single crystal substrate.6.2.1.1Select Open to open the window to edit the programparameters. For the Powder scans edit the 4 white boxes: Start angle, end angle, step size, and time per step.6.3Select the Repetition tab and ensure that the repetition is set to single6.3.1 Ensure the scan is set to Continuous6.3.2 The start angle MUST be larger than 5 degreesCAUTIONCAUTIONStart angles smaller than 5 degrees will cause the X-ray beamto shine directly into the detector and burn it out6.3.3 The max angle MUST be less than 140 degreesCAUTIONCAUTIONEnd angles larger than 140 degrees can cause the sourceand the detector to collide during the measurement

6.3.4 The step size will determine the resolution of your scan. Higherresolution will increase the scan quality but take longer to run. Thefollowing step sizes are offered as suggestions6.3.4.10.033 will run a quick scan (searching for peaks)6.3.4.20.016 will run a regular scan (general comparison)6.3.4.30.008 will run a high resolution scan (publication quality)6.3.4.40.002 is our max resolution with the X’Pert Powder6.3.5 The time per step will determine how long the software integrates ateach step. Larger values will reduce noise but will take longer toscan.6.3.5.16.3.5.2increase as neededYour main peak should be in the: 1000s of counts for peak ID 10,000s of counts for quantification 100,000s of counts for structure determination6.3.6 Leave all other parameters the sameYou should only needto adjust these 4boxes before savingthe programYour approximatescan time is shownhereEditing the scan parameters.6.4Click the close button (red X in the top right of the window) and selectsave changes6.5To run the program, select Measure - Program6.5.1 Select the same program you just saved6.5.2 This will open the measurement window6.6Select the large folder icon to choose where to save your scan data6.6.1 Data should be stored in the XRD User Data library in a folder withyour name

6.6.2 The folders and subfolders in your named directory can bewhatever you likeMeasurement window.Store all measurements in your folder in the XRD User Data library.6.7Before beginning the run, ensure the machine doors are completelyclosed6.8Select OK to begin the scan6.8.1 The tool will lock the doors. DO NOT attempt to open the doors.6.8.2 The scan will run autonomously at this point. A graph will pop upand plot data as it comes in. There is no alert when the scanfinishes. When all data is compiled, the machine will return the Xray source back to the start angle and unlock the doors.6.8.3 Once the doors are unlocked, you may proceed

7.0To stop a scan in progress7.17.2You can pause or stop a scan during data collection:Right-click within the scan display window SelectHold orStop7.3Or you can go to the top menu bar and click on the7.4The diffractometer will stop at its current position and give you an Optionsdialogue.The shutter will remain open until you choose an option7.5oricons.7.6You can choose to Abort the scan Data will be saved up to the point where youaborted the scan The diffractometer will move to its ‘park’ positionand the shutter will close Continue the scan The scan will resume from the point where youpaused it The system will wait as long as you want it to untilyou choose to continue8.0Sample Unloading8.0Once the doors are unlocked (there will be a loud click), you should besafe to open the door. However, ensure the X-ray is blocked with theindicator on the front of the machine.8.1If the X-ray is blocked (shutter is closed), open the doors slowly to retrieveyour sample.8.2If you are running additional samples, you may load them at this point,close the doors, and run more measurements8.3If you are finished with all your scans, remove all samples andloading/buffer slides from the machine and close the machine doors

9.0Post-Operation9.1When finished with the machine, you will need to return it to standbypower8.1.1 If someone is going to use the machine immediately after you andpower9.2Double click the current in the left window9.39.4Repeat until you reach 20mA (standby power)9.5Close all open windows in the Data Collector program, BUT DO NOTCLOSE THE DATA COLLECTOR PROGRAM ITSELF10.0 Converting Data10.1The tool stores data in its own proprietary format, which will include thescan parameters, which can be directly imported to the JCPDS computer.If you want an XY text file of data, use the following steps10.2Data Collector and Viewer programs in the Windows bar.10.3 In the window that opens, select File - Open10.4 Navigate to Libraries - XRD User Data - [your name] and select all).4.1Each scan will open its own window and an additional window willopen with all scans plotted on top of each other10.5 Select File - Convert All.5.1This process is quick, and the program does not acknowledgewhen it is finished.5.2Your XY files will be in the same folder as the original scans

Data Collector and Viewer programs in the Windows bar.10.6Close the data viewer program10.7Transfer your data files to a flash drive, you may leave data on thismachine, but it is periodically cleaned, and we are not responsible for lostdata.10.8You may transfer data to the JCPDS machine (will need a USB) to useHighScore Plus and the ICDD database to process your collected data.10.9At this point, you can log off at the TUMI computer

Panalytical XPert Powder X-Ray Diffraction SOP Table of Contents 1.0 Safety 2.0 Training 3.0 Sample Preparation 4.0 Pre-Operation 5.0 Sample Loading 6.0 Running a Measurement 7.0 To Stop a Scan in Progress 8.0 Sample Unl